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Dimethylformamide → 3-Methyl-1-phenyl-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

HRID 436414
ノート
印刷プレビュー

反応式

HRID 436414 の反応式
[C:1]1([N:7]2[C:12]3[N:13]=[CH:14][CH:15]=[CH:16][C:11]=3[CH2:10][NH:9][C:8]2=[O:17])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:18]N(C)C=O.[H-].[Na+].P(OC)(OC)(OC)=O>O>[C:1]1([N:7]2[C:12]3[N:13]=[CH:14][CH:15]=[CH:16][C:11]=3[CH2:10][N:9]([CH3:18])[C:8]2=[O:17])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 10541Trimethyl PhosphateHCID 24758Sodium hydrideHCID 132592811-Phenyl-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

生成物 1

HCID 132593543-Methyl-1-phenyl-3,4-dihydropyrido[2,3-d]pyrimidin-2(1H)-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 2.2 g of 1-phenyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine and 20 ml of dimethylformamide was added 0.5 g of approximately 50% sodium hydride, and the mixture was allowed to stand at room temperature for 30 minutes. To this was further added dropwise 4.2 g of trimethyl phosphate and the resulting mixture was heated at a temperature of 170° - 180° C in a sealed-tube for 7 hours. After the reaction was complete, the solvent was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was diluted with water, extracted with ether and dehydrated. The ether was removed by evaporation to leave a residue. This residue was recrystallized from a mixture of ether and petroleum ether to yield 1.7 g of 1-phenyl-3-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine as colorless prisms, melting at 172° - 173° C.

後処理

  1. temperaturethe resulting mixture was heated at a temperature of 170° - 180° C in a sealed-tube for 7 hours
  2. customthe solvent was removed from the reaction mixture by distillation under reduced pressure
  3. customThe residue thus obtained
  4. extractionextracted with ether
  5. customThe ether was removed by evaporation
  6. customto leave a residue
  7. customThis residue was recrystallized from a mixture of ether and petroleum ether

出典と根拠

ORDレコード
ord-b7cac1341ee94d228b974287d6d4fcab
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04009166

反応ノート

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